Nederlandse norm

NEN-EN 16857
(en)
Voedingsmiddelen - Bepaling van benzeen in
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frisdranken, andere dranken en

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zuigelingenvoeding op basis van groente met

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headspace gaschromatografie massa

spectrometrie (HS-GC-MS)
supplementary license agreement for use in a network with NEN has been concluded.

Foodstuffs - Determination of benzene in soft

drinks, other beverages and vegetable-based
infant foods by headspace gas chromatography
mass spectrometry (HS-GC-MS)

Vervangt NEN-EN 16857:2015 Ontw.

ICS 67.160.20; 67.230

mei 2017

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Als Nederlandse norm is aanvaard:

- EN 16857:2017,IDT

Normcommissie 370275 "Voedingsmiddelenanalyse - Horizontale methoden"

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EUROPEAN STANDARD EN 16857

NORME EUROPÉENNE
EUROPÄISCHE NORM May 2017

ICS 67.160.20; 67.230

English Version

Foodstuffs - Determination of benzene in soft drinks, other

beverages and vegetable-based infant foods by headspace
gas chromatography mass spectrometry (HS-GC-MS)
Produits alimentaires - Détermination de la teneur en
benzène dans les boissons non alcoolisées, les autres
boissons et les aliments pour nourrissons à base de
légumes par chromatographie en phase gazeuse avec
espace de tête couplée à la spectrométrie de masse (HS
CG-SM)
Lebensmittel - Bestimmung von Benzol in
Erfrischungsgetränken, anderen Getränken und in
Babynahrung auf Gemüsebasis mit Headspace-
Gaschromatographie/Massenspektrometrie (HS-GC-
MS)

This European Standard was approved by CEN on 20 February 2017.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 16857:2017 E
worldwide for CEN national Members.

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Contents Page

European foreword....................................................................................................................................................... 3
1 Scope .................................................................................................................................................................... 4
2 Normative references .................................................................................................................................... 4
3 Principle ............................................................................................................................................................. 4
4 Reagents ............................................................................................................................................................. 4
5 Apparatus........................................................................................................................................................... 6
6 Procedure........................................................................................................................................................... 8
7 HS-GC-MS analysis........................................................................................................................................... 8
8 Calculation ...................................................................................................................................................... 11
9 Precision data ................................................................................................................................................ 11
10 Test report ...................................................................................................................................................... 12
Annex A (informative) Typical chromatograms ............................................................................................ 13
Annex B (informative) Precision data ............................................................................................................... 14
Bibliography ................................................................................................................................................................. 15

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European foreword

This document (EN 16857:2017) has been prepared by Technical Committee CEN/TC 275 “Food
analysis - Horizontal methods”, the secretariat of which is held by DIN.

This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by November 2017, and conflicting national standards
shall be withdrawn at the latest by November 2017.

Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document has been prepared under a mandate given to CEN by the European Commission and the
Europan Free Trade Association.

WARNING — The use of this standard can involve hazardous materials, operations and
equipment. This standard does not purport to address all the safety problems associated with its
use. It is the responsibility of the user of this standard to take appropriate measures for
ensuring the safety and health of the personnel prior to application of the standard and to fulfil
statutory requirements for this purpose. Benzene has been classified by IARC as carcinogenic to
humans (see [1]).

According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.

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1 Scope
This European Standard specifies a method for the determination of benzene in soft drinks, other
beverages and vegetable-based infant foods, by headspace gas chromatography mass spectrometry (HS-
GC-MS). The method has been validated in an interlaboratory study via the analysis of spiked samples of
carbonated soft drink, still fruit-based drink, carbonated fruit-based drink, vegetable and fruit juice
containing carrot, infant food vegetable based and infant food containing meat, ranging from 1,9 µg/kg
to 18,6 µg/kg. However, linearity of the instrument response was proven for the concentration range
from 0,5 µg/kg to 20 µg/kg. The limit of quantification (LOQ) depends on the instrument but can
generally be expected to be in the range from 0,5 µg/kg to 1,0 µg/kg.

2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 3696:1995, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987)

3 Principle
The sample is homogenized, a test portion is heated in a closed system with isotopically-labelled
benzene added as internal standard. A portion of the headspace is injected into a GC-MS system for
identification and quantification. The injection is performed with a split-splitless injection port. The
chromatographic separation is obtained on a mid-polarity capillary GC column. The benzene is ionized
at 70 eV, recorded in selected ion monitoring (SIM) mode, and quantified by comparison with the stable
isotope labelled analogue.

4 Reagents
Use only reagents of recognized analytical grade and water complying with grade 1 of
EN ISO 3696:1995, unless otherwise specified. Prepare standard solutions preferably gravimetrically.
Use an analytical balance (5.1) for the preparation of both native and stable isotope labelled benzene
standard solutions.
4.1 Benzene, C6H6, purity is ≥ 99,0 % (CAS 71-43-2).

While not necessary, it is recommended to store at 4 °C to 6 °C to prevent evaporation. Bring to room

temperature before use.
4.2 Benzene-d6, purity is ≥ 99, 6 atom % D (CAS 1076-43-3).

While not necessary, it is recommended to store at 4 °C to 6 °C to prevent evaporation. Bring to room

temperature before use.
4.3 Helium purified compressed gas, purity equivalent to 99,995 % or better.

4.4 Methanol, suitable for headspace GC analysis (CAS 67-56-1).

4.5 Preparation of stock and standard solutions

4.5.1 General

Prepare all standard solutions preferably gravimetrically. Record the tare masses of all recipients and
the masses after each preparation step and use for calculation of the mass concentrations of standard
solutions.

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Volumetric preparation of standard solutions may also be applied provided that the volumetric
glassware used complies with EN ISO 1042 (see [2]).
4.5.2 Benzene stock solution, mass concentration ρ approximately 2,20 mg/ml

Pipette 20 ml ± 0,1 ml of methanol into a 20 ml headspace vial (5.17) and seal the vial with a crimp cap.
Weigh the sealed vial to the nearest 0,1 mg and record the weight as W1. Using a microsyringe, transfer
50 µl of benzene (4.1) through the septum of the vial containing the methanol and shake vigorously or
vortex to mix. Reweigh the sealed vial and record the weight (W2) to the nearest 0,1 mg. Subtract W1
from W2 to determine the weight of benzene transferred (W3). Calculate the mass concentration of stock
solution from W3 divided by the total volume (20,05 ml).
Alternatively, commercially available certified standard solutions may be used if available. Store the
benzene stock solution at 4 °C to 6 °C but allow it to attain ambient temperature before use. Discard
after 2 weeks. Once the septum on the stock solution has been pierced, the cap shall be replaced.
4.5.3 Benzene intermediate standard solution, ρ approximately 54 µg/ml

Using a microsyringe, transfer 500 µl of benzene stock solution (4.5.2) to a sealed headspace vial
containing 20 ml ± 0,1 ml of methanol and shake vigorously. Prepare fresh daily. Calculate the exact
mass concentration from the stock solution (4.5.2).
4.5.4 Benzene standard solution, ρ approximately 0,5 µg/ml

Using a microsyringe, transfer 200 µl of benzene intermediate standard solution (4.5.3) to a sealed
headspace vial containing 20 ml ± 0,1 ml of water and shake vigorously. Prepare fresh daily. Calculate
the exact concentration from the stock solution (4.5.2). Use this standard solution to prepare a 6-point
calibration from 0,5 µg/kg to 20 µg/kg (see 4.6).
4.5.5 Benzene-d6 internal standard (IS) stock solution, ρ approximately 2,36 mg/ml

Pipette 20 ml ± 0,1 ml of methanol into a 20 ml headspace vial (5.17) and seal the vial with a crimp cap.
Weigh the sealed vial to the nearest 0,1 mg and record the weight as W1. Using a microsyringe, transfer
50 µl of benzene-d6 (4.2) through the septum of the vial containing the methanol and shake vigorously
or vortex. Reweigh the sealed vial and record the weight (W2) to the nearest 0,1 mg. Subtract W1 from
W2 to determine the weight of benzene-d6 transferred (W3). Calculate the mass concentration of IS stock
solution from W3 divided by the total volume (20,05 ml).
Alternatively, commercially available certified standard solutions may be used if available. Store the
benzene-d6 IS stock solution at 4 °C to 6 °C but allow it to attain ambient temperature before use.
Discard after 2 weeks. Once the septum on the IS stock solution has been pierced, the cap shall be
replaced.
4.5.6 Benzene-d6 internal standard (IS) solution, ρ approximately 4,2 µg/ml

Using a microsyringe, transfer 36 µl of benzene-d6 IS stock solution (4.5.5) to a sealed headspace vial
containing 20 ml ± 0,1 ml of water and shake vigorously. Prepare fresh daily. Calculate the exact mass
concentration from the benzene-d6 IS stock solution (4.5.5).
4.6 Preparation of the calibration solutions

Prepare calibration solutions of approximately 0 µg/kg, 0,5 µg/kg, 1 µg/kg, 2,5 µg/kg, 5 µg/kg, 10 µg/kg
and 20 µg/kg benzene and approximately 10 µg/kg IS according to the following scheme.
Add 10 g ± 0,05 g of water to each of seven 20 ml headspace vials and transfer using a positive
displacement pipette benzene standard solution (4.5.4), IS solution (4.5.6)and water according to the
values given in Table 1. To avoid loss of benzene, seal the vials immediately following addition of the
entire benzene and benzene-d6 solutions and water.

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Table 1 — Preparation of calibration solutions

Mass of Volume of Volume of Volume of

Benzene d6
water 0,5 µg/ml 4,2 µg/ml water Benzene mass
mass
g benzene benzene-d6 µl concentration
concentration
(4.5.4) (4.5.6) µg/kg
µg/kg
µl µl
10 0 25 400 0 10,1
10 10 25 390 0,5 10,1
10 20 25 380 1,0 10,1
10 50 25 350 2,5 10,1
10 100 25 300 5,0 10,1
10 200 25 200 10 10,1
10 400 25 0 20 10,1

5 Apparatus
WARNING — All glassware shall be meticulously cleaned (except disposable glassware).
Usual laboratory glassware and equipment and, in particular, the following:
5.1 Analytical balance, capable of weighing to the nearest of 0,0 001 g.

5.2 Top pan balance, capable of weighing to the nearest 0,001 g.

5.3 Headspace gas chromatography – mass spectrometry (HS-GC-MS) apparatus, comprising the
following:

5.3.1 Headspace sampling and injection system, suitable for incubation temperatures of up to
60 °C and incubation time of 30 min. The headspace sampling needle should be suitable for
maintenance at 100 °C and the transfer line at 105 °C.

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5.3.2 Injection system, split-splitless injector, suitable for temperatures up to 250 °C.

A programmed temperature vaporizing (PTV) injector may be used as an alternative to a split/splitless

injector. However, split/splitless injection was proven in the method validation study by collaborative
trial suitable for the scope of this standard.
5.4 GC oven, suitable for temperatures up to 240 °C and capable of temperature programming.

5.5 Sample carousel, suitable for use with 20 ml glass headspace vials and caps (5.17).

5.6 GC capillary column, DB-VRX 1) 6 %-cyanopropylphenyl-94 %-dimethylpolysiloxane length of

60 m, internal diameter of 0,25 mm, df = 1,4 µm (β = 44), or any column with comparable separation
characteristics.

5.7 Interface to the mass spectrometer, with a temperature control device, suitable for
temperatures up to 250 °C.

5.8 Mass spectrometer with the following characteristics:

— electron ionization source;

— ionization energy of 70 eV;

— mass resolution of at least 1 at each prescribed m/z value;

— temperature control devices for the ion source (230 °C) and the GC-MS interface (225 °C).
Optionally a temperature control device for the quadrupole (150 °C);

— tuning stability of at least 48 h (allowing for the analysis of a sequence of samples and standards);

— response linearity range of at least two orders of magnitude.

5.9 Computer based instrument control system, capable of programming headspace sampling, gas
chromatographic and mass spectrometric acquisition depending upon run time.

5.10 Data processing system, computer based.

5.11 Crimper, for sealing vial caps (5.17).

5.12 De-crimper, for removing vial caps (5.17).

5.13 Oven, forced-air maintained at 90 °C ± 1 °C.

5.14 Pipettes, glass, 10 ml and 20 ml capacity.

5.15 Pipettes, calibrated positive displacement, 10 µl to 400 µl capacity.

5.16 Syringes, calibrated precision glass, 50 µl, 100 µl, 250 µl and 500 µl capacity.

1) This is an example of a suitable product available commercially. This information is given for the convenience
of users of this European Standard and does not constitute an endorsement by CEN of this product. Equivalent
products may be used if they can be shown to lead to the same results.

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5.17 Vials, glass, for headspace analysis, 20 ml capacity with aluminium crimp seals and PTFE-faced
silicon septa. If necessary, dry the vials at 90 °C ± 1 °C in a forced-air oven for approximately 1 h and
cool to ambient temperature.

6 Procedure
6.1 General

Benzene formation can occur in soft drinks (and other foodstuffs) containing benzoate salts,
particularly those with added ascorbic acid, when exposed to elevated temperatures and/or UV light. In
order to exclude changes in benzene levels, the analysis should be performed within as short a period
as possible after sample reception. Samples should be stored under appropriate temperature conditions
and excluded from light. There is no evidence to suggest that benzene is formed during analysis using
this procedure.
6.2 Sample treatment

Samples are processed in duplicate. As a general precaution, all of the sample material received by the
laboratory shall be used for obtaining a representative and homogeneous laboratory sample without
introducing secondary contamination.
Allow frozen samples to defrost fully by storing in a refrigerator (4 °C to 6 °C) overnight, then allow
them to reach room temperature before carrying out the following steps.
6.3 Test sample preparation

To obtain the test sample and avoid loss of benzene, quickly weigh 10 g ± 0,01 g portions of sample into
tared headspace vials, add 25 μl of the benzene-d6 internal standard solution (ρ approximately
4,2 μg/ml) (4.5.6) and 400 µl of water, securely cap the vial, and mix by adequate shaking or vortexing.
For some solid samples it may be necessary to slurry the sample with water at a sample to water ratio
of 1:1 to obtain a suitably mobile product e.g. 5 g ± 0,005 g of sample slurried in 5 ml ± 0,005 ml of
water. This process will effectively increase the LOQ by a factor of 2 and the consequent dilution shall
be accounted for in the final calculation of benzene content as described in Clause 8.

7 HS-GC-MS analysis
7.1 General

Set up the HS-GC in accordance with the manufacturer’s instructions and optimize the conditions for the
analysis of benzene. Example conditions and chromatographic system suitability criteria are given in
Annex A.
Satisfactory separation of benzene and other volatile components in the sample is obtained with the
gas-chromatographic column (5.6) and the following settings. However, the given parameters may not
be acceptable with all types of instruments. Modifications and optimizations may be required for the
achievement of satisfactory chromatographic separation.
Headspace injection volume and injector split ratio should be determined specifically for the instrument
used. Timed-mode injection may also be used. If the temperature and time of the sample incubation are
changed, the efficacy of the method shall be determined.

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7.2 Headspace sampling conditions

— incubation temperature: 60 °C ± 1 °C;

— incubation time: 30 min;

— needle temperature: 100 °C;

— transfer line temperature: 105 °C;

— injection time: 1 min.

7.3 Injection conditions for split/splitless injector

— inlet temperature: 200 °C;

— split ratio: 10:1;

— injection volume: 1 ml.

7.4 Oven conditions

— initial temperature: 40 °C;

— initial time: 3 min;

— first ramp: 10 °C/min up to 240 °C;

— static time: 3 min.

7.5 Column conditions

— carrier gas flow: 1,2 ml/min, constant flow;

— carrier gas type: Helium.

7.6 Transfer line conditions

— temperature: 225 °C.

7.7 Mass spectrometer conditions

— MS source temperature: 230 °C;

— MS quadrupole temperature: 150 °C;

— electron ionization energy: 70 eV.

7.8 Mass spectrometer acquisition parameters and peak identification

The acquisition of the m/z signals is performed in SIM mode according to Table 2. For quantification of
benzene, the peak area of the quantifier ion is used. However, the benzene peak is only considered
identified when the qualifier ions are also present and the peak area ratios between the quantifier and
qualifier ions are in the acceptable range. Commission Decision 2002/657/EC may be used for guidance
on acceptable peak area ratios (see [3]).

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Table 2 — Acquisition parameters in SIM mode

Compound Observed ions

m/z
51: [C4H3]+ Identification only

Benzene 77: [C6H5]+ Identification only

78: [C6H6]+ Identification and quantification

52: [C4D2]+ Identification only
Benzene-d6
84: [C6D6]+ Identification and quantification
7.9 Calibration curve

Inject the calibration solutions listed in Table 1 at the beginning of every sequence. All solutions shall be
incubated according to the conditions given in 7.2. The injection of the calibration solutions shall be
performed from the lower to the higher concentration in order to reduce the risk of cross-
contamination.
The calibration curve is obtained by plotting the peak area ratio of benzene and the benzene-d6 internal
standard against the concentration ratio of benzene and the benzene-d6 in the calibration solutions.
The calibration function is defined by linear regression, and is described by Formula (1):
Am/ z 78 w benzene
a×
= +b (1)
Am/ z 84 w benzene − d 6

where
Am/z 78 is the peak area of the benzene quantifier ion (m/z 78);
Am/z 84 is the peak area of the benzene-d6 quantifier ion (m/z 84);
a is the slope of the calibration curve;
b is the intercept of the calibration curve;
wbenzene is the mass fraction of benzene in the calibration solution, in µg/kg;
wbenzene-d6 is the mass fraction of benzene-d6 in the calibration solution, in µg/kg.
The calibration curve shall not be forced through the origin.
7.10 Sample analysis

Each sequence encompasses besides calibration samples and sample extracts, a procedural blank
sample.
A procedural blank is a blank sample made up of all reagents foreseen for preparation of a test portion
and processed in all respects as a test portion. This kind of blank tests the purity of the reagents as well
as other possible sources of contamination such as glassware and the analytical instrumentation. The
procedural blank comprises 10 g ± 0,01 g plus 400 µl of water and 25 μl of the benzene-d6 internal
standard solution (ρ approximately 4,2 μg/ml) (4.5.6).
Before starting the sequence, evaluate the system suitability based on at least one solvent blank sample.
Inject the calibration solutions in order of increasing concentration. Additional solvent blank samples
may be added in the sequence whenever the analyst considers it necessary.

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For large analytical batches of 10 samples or above, the batch should be interspersed with a midlevel
calibration solution, e.g. 10 µg/kg as a quality control check after every 10 samples.

8 Calculation
Calculate the benzene mass fraction of the sample, w, in µg/kg, using Formula (2):
 Am/ z 78 
 −b
 Am/ z 84 
  (2)
=w ×f
a

where
a is the slope of the calibration curve, see 7.9;
b is the intercept of the calibration curve, see 7.9;
f is the dilution factor applied if the sample was slurried with water beforehand (here: f = 2,
see 6.3).
The result reported will be the average of two replicate measurements performed for the particular test
sample. Report the analysis result to the nearest 0,10 µg/kg. In case the analyte content is below the
limit of detection (LOD) or the limit of quantitation (LOQ) report the results below the LOD or below the
LOQ respectively, and provide the concentrations corresponding to the LOD and LOQ of the method
accordingly.
If the calculated benzene content exceeds the upper limit of the working range, re-analyse the sample
with an adjusted, lower sample intake by diluting liquid samples with water or by slurrying solid
samples in water, and making a note of the dilution factors used.

9 Precision data
9.1 General

Details of the interlaboratory test of the precision of the method are summarized in Annex B. The values
derived from the interlaboratory test may not be applicable to analyte concentration ranges and/or
matrices other than those given in Annex B.
9.2 Repeatability

The absolute difference between two single test results found on identical test material by one operator
using the same apparatus with the shortest feasible time interval will exceed the repeatability limit r in
not more than 5 % of the cases.
The values for benzene are:
x̅ = 3,1 µg/kg r = 0,86 µg/kg (water)
x̅ = 18,6 µg/kg r = 2,47 µg/kg (carbonated soft drink)
x̅ = 1,9 µg/kg r = 1,05 µg/kg (still fruit-based drink)
x̅ = 2,0 µg/kg r = 0,11 µg/kg (carbonated fruit-based drink)
x̅ = 2,0 µg/kg r = 0,95 µg/kg (vegetable / fruit juice containing
carrot)
x̅ = 4,3 µg/kg r = 0,36 µg/kg (infant food vegetable based)
x̅ = 2,2 µg/kg r = 0,98 µg/kg (infant food containing meat)

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9.3 Reproducibility

The absolute difference between two single test results found on identical test material reported by two
laboratories will exceed the reproducibility limit R in not more than 5 % of the cases.
The values for benzene are:
x̅ = 3,1 µg/kg R = 2,66 µg/kg (water)
x̅ = 18,6 µg/kg R = 13,59 µg/kg (carbonated soft drink)
x̅ = 1,9 µg/kg R = 2,15 µg/kg (still fruit-based drink)
x̅ = 2,0 µg/kg R = 0,47 µg/kg (carbonated fruit-based drink)
x̅ = 2,0 µg/kg R = 3,38 µg/kg (vegetable / fruit juice containing carrot)
x̅ = 4,3 µg/kg R = 5,29 µg/kg (infant food vegetable based)
x̅ = 2,2 µg/kg R = 3,28 µg/kg (infant food containing meat)

10 Test report
The test report should contain the data according to ISO/IEC 17025 [4] and shall contain the following
data:
a) all information necessary for the identification of the sample (type of sample, origin and
designation of the sample);

b) a reference to this European Standard;

c) the date and type of sampling procedure (if known);

d) the date of receipt;

e) the date of test;

f) the test results and the units in which they have been expressed;

g) any operations not specified in the method or regarded as optional, which might have affected the
results.

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Annex A
(informative)

Typical chromatograms

a) b)
Key
a) benzene Y abundance
b) benzene-d6 t time in min
Operating conditions:

— capillary column DB-VRX 6 %-cyanopropylphenyl-94 %-dimethylpolysiloxane length of 60 m,

internal diameter of 0,25 mm, df = 1,4 µm, β = 44;

— temperature programme: 40 °C for 3 min, then 10 °C/min to 240 °C and hold 3 min;

— carrier gas flow: 1,2 ml/min helium (constant flow = 28 cm/s).

Figure A.1 — Typical chromatograms of benzene (a) and benzene-d6 (b)

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Annex B
(informative)

Precision data

The data given in Table B.1 were obtained in an interlaboratory study, organized by the Food and
Environment Research Agency, UK (Fera), in accordance with ISO 5725-2 [4] for collaborative study
procedures to validate characteristics of a method of analysis and Thompson with regard to
interlaboratory precision at analyte concentrations below 120 mg/kg (see [5]).
Table B.1 — Precision data for benzene in beverages and vegetable-based infant food by
headspace GC-MS

Sample 1 2 3 4 5 6 7
Preparation of test material spiked spiked spiked spiked spiked spiked spiked

Year of interlaboratory test 2014 2014 2014 2014 2014 2014 2014
Number of laboratories 9 9 9 9 9 9 9
Laboratories considered as non-
0 1 1 1 1 1 1
compliant
Number of outliers (laboratories) 0 0 0 2 0 1 0
Number of accepted results 9 8 8 6 8 7 8
Mean value, x̅ , µg/kg 3,1 18,6 1,9 2,0 2,0 4,3 2,2
Repeatability standard deviation sr,
0,31 0,88 0,38 0,04 0,34 0,13 0,35
µg/kg
Repeatability relative standard
9,8 4,7 19,5 13,6 17,3 3,0 15,7
deviation, RSDr, %
Repeatability limit r [r = 2,8 × sr ],
0,86 2,47 1,05 0,11 0,95 0,36 0,98
µg/kg
Reproducibility standard deviation
0,95 4,85 0,77 0,17 1,21 1,89 1,17
sR, µg/kg
Reproducibility relative standard
30,2 26,1 40,0 55,6 61,3 44,3 52,5
deviation, RSDR, %
Reproducibility limit R
2,66 13,59 2,15 0,47 3,38 5,29 3,28
[R = 2,8 × sR], µg/kg
HorRat value, according to [5] 1,4 1,2 1,8 2,5 2,8 2,0 2,4
1 Water, pre-trail sample, 2 Carbonated soft drink, 3 Still fruit-based drink, 4 Carbonated fruit-based
drink, 5 Vegetable/fruit juice containing carrot, 6 Infant food vegetable based, 7 Infant food
containing meat

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Bibliography

[1] International Agency for Research on Cancer. IARC Monograph on the evaluation of carcinogenic
risk to humans, Volume 100F, Benzene

[2] EN ISO 1042:1999, Laboratory glassware - One-mark volumetric flasks (ISO 1042:1998)

[3] 2002/657/EC – Commission Decision of 12 August 2002 implementing Council Directive

96/23/EC concerning the performance of analytical methods and the interpretation of results.
Official Journal of the European Communities, 17.8.2002, L221/8-36

[4] ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories

[5] ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results —
Part 2: Basic method for the determination of repeatability and reproducibility of a standard
measurement method

[6] THOMPSON M., Recent trends in inter-laboratory precision at ppb and sub-ppb concentrations in
relation to fitness for purpose criteria in proficiency testing. Analyst (Lond.). 2000, 125 pp. 385–
386

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Waarom betaalt u voor een norm?
Normen zijn afspraken voor en door de markt, zo ook deze norm. NEN begeleidt het gehele
normalisatieproces. Van het bijeenbrengen van partijen, het maken en vastleggen van de afspraken en het
bieden van hulp bij de toepassing van de normen. Om deze diensten te kunnen bekostigen betalen alle
belanghebbende partijen die aan tafel zitten voor het normalisatieproces, en u als gebruiker voor normen en
trainingen. NEN is een stichting en heeft geen winstoogmerk.

Wat is nu precies de toegevoegde waarde van normen?

Stelt u zich eens voor … u wilt in het buitenland geld pinnen, maar uw bankpas past niet. Of uw nieuwe
telefoon herkent uw simkaart niet. De samenstelling van de benzine over de grens is anders waardoor u niet
kunt tanken. Het dagelijks leven zou zonder goede afspraken over producten, processen en diensten een stuk
complexer zijn.

Het maken en vastleggen van afspraken door belanghebbende partijen noemen we het normalisatieproces.
Normalisatie had vanouds betrekking op techniek en producten. Nu worden steeds vaker normen voor
diensten ontwikkeld. Zo zijn er afspraken op het gebied van gezondheidszorg, schuldhulpverlening,
kennisintensieve dienstverlening, externe veiligheid en MVO.

Normen zorgen voor verbetering van producten, diensten en processen; qua veiligheid, gezondheid,
efficiëntie, kwaliteit en duurzaamheid. Dit ziet u op de werkvloer, in de omgang met elkaar en in de
samenleving als geheel. Organisaties die normalisatie onderdeel van hun strategie maken, vergroten hun
professionaliteit, betrouwbaarheid en concurrentiekracht.

Wat doet NEN?

NEN ondersteunt in Nederland het normalisatieproces. Als een partij zich tot NEN richt met de vraag om een
afspraak tot stand te brengen, gaan wij aan de slag. We onderzoeken in hoeverre normalisatie mogelijk is en
er interesse voor bestaat. Wij nodigen vervolgens alle belanghebbende partijen uit om deel te nemen. Een
breed draagvlak is een randvoorwaarde. De afspraken komen op basis van consensus tot stand en worden
vastgelegd in een document. Dit is meestal een norm. Afspraken die in een NEN-norm zijn vastgelegd mogen
niet conflicteren met andere geldige NEN-normen. NEN-normen vormen samen een coherent geheel. Een
belanghebbende partij kan een producent, ondernemer, dienstverlener, gebruiker, maar ook de overheid of
een consumenten- of onderzoeksorganisatie zijn. De vraag is niet altijd om een norm te ontwikkelen. Vanuit
de overheid komt regelmatig het verzoek om te onderzoeken of er binnen een bepaalde sector of op een
bepaald terrein normalisatie mogelijk is. NEN doet dan onderzoek en start afhankelijk van de uitkomsten een
project. Deelname staat open voor alle belanghebbende partijen. NEN beheert ruim 30.000 normen. Dit zijn
de in Nederland aanvaarde internationale (ISO, IEC), Europese (EN) en nationale normen (NEN). In totaal zijn
er ruim 800 normcommissies actief met in totaal bijna 5.000 normcommissieleden. Een goed beheer van de
omvangrijke normencollectie en de afstemming tussen nationale, Europese en internationale
normcommissies vereisen dan ook een zeer goede infrastructuur.

Betalen kleine organisaties net zoveel als grote organisaties?

Het uitgangspunt is dat alle partijen die deelnemen aan het normalisatieproces een evenredig deel betalen.
De normcommissieleden kunnen onderling andere afspraken maken. Zo worden er wel eens afspraken
gemaakt dat de grote partijen een groter deel betalen dan de kleinere bedrijven. De prijzen voor normen zijn
voor iedereen gelijk. De kosten voor licenties zijn afhankelijk van de omvang van een organisatie en het
aantal gebruikers.

Voordelen van normalisatie en normen

Gegarandeerde kwaliteit | Veiligheid geborgd | Bevordert duurzaamheid | Opschalen en vermarkten van
nieuwe innovatieve producten | Meer (internationale) handelsmogelijkheden | Verhoogde effectiviteit en
efficiëntie | Onderscheidend in de markt.

Voordelen van deelname

Invloed op de (internationale en Europese) afspraken | Als eerste op de hoogte van veranderingen | Netwerk;
ook op Europees en internationaal niveau | Kennisvergroting.

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